Lewis-Base Adducts of Group 11 Metal(I) Compounds. XXIV. 1:2 Silver(I) Halide/Monodentate Amine Complexes: A Novel Structural Type in 1-2 Silver(I) Chloride Piperidine

1988 ◽  
Vol 41 (3) ◽  
pp. 417 ◽  
Author(s):  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Silver Atom ◽  
Structural Type ◽  
Lewis Base ◽  
One Dimensional ◽  
X Ray ◽  
Amine Complexes

Recrystallization of silver(I) chloride from neat piperidine (L) yields a 1 : 2 adduct, characterized by a single-crystal X-ray study. Crystals are monoclinic, C2/c, a 20.76(4), b 6.422(7), c 20.69(2)Ǻ, β 96.9(1)°, Z 8; R 0.042 for 1061 'observed' reflections. The structure, the first determined for a 1 : 2 silver(I) chloride/monodentate amine adduct, is an infinite one-dimensional chloro-bridged polymer -AgL2-Cl-AgL2-Cl-. About the four-coordinate silver atom, Ag-Cl are 2.524(3), 2.667(3)Ǻ, Ag-N 2.385(9), 2.347(11)Ǻ, with Ag-Cl-Ag 102.62(9)°; the largest angle in the silver environment is 120.3(2)°(Cl-Ag-N).

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXXIV Synthesis and Structure of the 1 : 1 Adduct of Silver(I) Nitrate with Triphenylstibine

1997 ◽  
Vol 50 (6) ◽  
pp. 671 ◽  
Author(s):  
Effendy ◽  
John D. Kildea ◽  
Allan H. White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Related Species ◽  
Room Temperature ◽  
Structural Data ◽  
Lewis Base ◽  
One Dimensional ◽  
X Ray ◽  
The One

The synthesis and room-temperature single-crystal X-ray structure determination of the 1 : 1 adduct of silver(I) nitrate with triphenylstibine, AgNO3/SbPh3 (1 : 1), is recorded, being monoclinic, Cc,a 12·824(2), b 15·794(4),c 9·796(2) Å, β 117·50(1)°, Z= 4; conventional R on F was 0·030 for 2881 independent ‘observed’ (I > 3σ(I)) reflections. The complex is a one-dimensional polymer with bridging nitrate groups, resembling in this respect its phosphine and arsine analogues. The completion of this study, along with related species recorded in accompanying papers, means that full structural data are now available for the complete array AgNO3/EPh3 (1 : n), E = P, As, Sb, n = 1–4, with the one exception of E = Sb, n = 2.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. XL. Conformational Systematics of [(N-base)1(CuX)1]∞ Orthogonal' Stair' Polymers (N-base = 'One-Dimensional Aceto-nitrile, Benzo-nitrile Ligand)

1989 ◽  
Vol 42 (1) ◽  
pp. 79 ◽  
Author(s):  
PC Healy ◽  
JD Kildea ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Polymer Chain ◽  
Structural Chemistry ◽  
Lewis Base ◽  
One Dimensional ◽  
X Ray ◽  
The Common ◽  
Reference Parameters ◽  
Polymer Type

The structural chemistry of the polymeric 1:1 adducts of copper(1) halides ( CuX ; X = Cl, Br, I) with nitrile bases (exemplified by aceto- and benzo-nitrile ) has been systematically explored. Single-crystal X-ray structure redeterminations of enhanced precision have been carried out for all acetonitrile adducts (refined as orthorhombic, Pbnm , Z 4, a ≈ 13.0, b ≈ 8.5, c ≈ 4.0 � ; R 0.039, 0.030, 0.043 for No = 534, 365, 727 'observed' reflections) and the chloride and bromide benzonitrile adducts (monoclinic, P21/n, a ≈ 3.9, b ≈ 17.5, c ≈10.9 � , β ≈ 98, Z 4); R 0.046, 0.048 for No = 1452, 1209); all structures are of the common one-dimensional 'stair' polymer type. In these adducts, the ligand is essentially 'one-dimensional' with substituents well removed from the point of attachment and from interaction within the parent polymer chain. Under these circumstances, the polymer is essentially 'orthogonal' with Cu-X crosslinks at (or nearly at) right angles to the polymer axis, and containing quasi-mirror planes, the series providing reference parameters for the description of distortions observed in these polymers when more hindered bases are coordinated.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LII. Synthesis and Structural Characterization of Mononuclear Chloro- and Bromo-pyridinebis-(triphenylphosphine)silver(I) Complexes

1989 ◽  
Vol 42 (6) ◽  
pp. 907 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Silver Atom ◽  
Lewis Base ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Weak Coordination

The mononuclear adducts chloro - and bromo-pyridinebis (triphenylphosphine)silver have been synthesized and structurally characterized by single-crystal X-ray diffraction methods. The two complexes are isomorphous, monoclinic, space group P21 or P21/m, a ≈ 9.8, b ≈ 20.0, c ≈ 9.1 � , β ≈ 97.5�, Z 2; in space group P21/m, they were refined to residuals of 0.038, 0.036 for 2392, 2157 'observed' reflections respectively. No comparable iodide adduct has been isolated. In both structures the silver atom is four-coordinate; Ag-Cl,Br are 2.511(2), 2.629(1) �; Ag-P, 2.472(1), 2.476(1) �, and Ag-N, 2.585(5), 2.570(5) � respectively, the Ag-N distance being longer than Ag-P, indicating very weak coordination of the pyridine.

Lewis-Base Adducts of Lead(II) Compounds. VII. Synthetic and Structural Studies of Some 1:1 Adducts of Linear Polyamines With Lead(II) Nitrate

1996 ◽  
Vol 49 (10) ◽  
pp. 1029 ◽  
Author(s):  
JM Harrowfield ◽  
H Miyamae ◽  
BW Skelton ◽  
AA Soudi ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Coordination Sphere ◽  
Room Temperature ◽  
Internal Symmetry ◽  
Lewis Base ◽  
Structural Studies ◽  
One Dimensional ◽  
X Ray ◽  
Structure Determinations

Syntheses and room-temperature single-crystal X-ray structure determinations are recorded for 1 : 1 adducts of lead(II) nitrate with the linear multidentate polyamines ethane-1,2-diamine ('en'(= '2')), H2N(CH2)2NH(CH2)2NH2(' dien ' = '22') and H2N(CH2)xNH(CH2)yNH(CH2)zNH2 ( xyztet = '222tet' (= ' trien '), '232tet', '323tet'). Crystal/refinement data are as follows: [(en) Pb (NO3)2](∞|∞) is monoclinic, P 21/c, a 5.388(2), b 12.440(5), c 13.123(3) Ǻ, β 102.33(3)°, Z = 4 f.u .; R 0.037 for No 2698 'observed' (I > 3σ(I)) reflections. [( dien ) Pb (NO3)2](∞|∞) is orthorhombic, Ccma , a 9.800(2), b 10.840(2), c 20.521(5), Z = 8; R 0.045, No 991. [( trien ) Pb (NO3)2](∞|∞) is orthorhombic, P 212121, a 14.815(3), b 10.975(3), c 8.410(2) Ǻ, Z = 4; R 0.050, No 1360; [(232tet) Pb (NO3)2](∞|∞) is isomorphous, a 14.524(6), b 11.221(1), c 8.860(2) Ǻ, R 0.036, No 2371. [(323tet) Pb (NO3)2](∞|∞) is monoclinic, P21/c, a 8.195(4), b 14.407(7), c 13.312(4) Ǻ, β 91.05(3)°, Z = 4; R 0.049, No 1644. In general, the degree of complexity of the adduct diminishes as the ligand size increases: whereas the en adduct is a compact one-dimensional two stranded polymer with nearly all nitrate oxygens involved in tight bridging interactions, the extent of bridging diminishes in the adducts of the larger amines, until, for the 323tet species, a monomer is obtained involving a lead coordination sphere containing the ligand and a pair of bidentate nitrate groups. The 1 : 2 adduct with en is also recorded, and is a dimer with quasi-i internal symmetry. [(en)2Pb(NO3)2]2 is monoclinic, P21, a 6.661(2), b 14.226(8), C 13.618(4)Ǻ, β 96.51(2)°; R 0.072, No 1713.

Lewis-base adducts of Group 1B metal(I) compounds. VII. Synthesis and structures of the 1 : 1 adducts of copper(I) halides with N,N,N',N'-tetramethyletlrylenediamine

1984 ◽  
Vol 37 (11) ◽  
pp. 2207 ◽  
Author(s):  
LM Engelhardt ◽  
RI Papasergio ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
X Ray

1 : 1 adducts of N,N,N',N'-tetramethylethylenediamine ('tmeda') with copper(1) chloride, bromide and iodide have been synthesized and the structures of the solid iodide and chloride derivatives established by single-crystal X-ray diffraction methods. The iodide,(1),is monoclinic, P21/c, a 12.370(5), b 12.119(5), c 15.36(1) �, β 109.16(5)�, Z = 4 dimers; the residual R was 0.067 for 1240 'observed' reflections. The complex is a ��'-diiodobridged dimer (tmeda)CuI2Cu(tmeda); thedistance between the pair of four-coordinate copper atoms is very short [2.566(4) A]. The bromide is isomorphous with the iodide. The chloride, (2), is monoclinic, P21/n, a 14.477(3), b 15.063(3),c 9.326(2) �, β 96.99(2)�, Z = 4 formula units; R was 0.055 for No = 1195. The complex is ionic [Cu(tmeda)2]+ [CuCl2]-.

Synthesis, IR spectrum, thermal behaviour and crystal structure of a novel one-dimensional cyano-bridged zinc(II)/nickel(II) complex

2005 ◽  
Vol 220 (1) ◽  
Author(s):  
Ahmet Karadag ◽  
Hümeyra Pasaoglu ◽  
Gökhan Kastas ◽  
Orhan Büyükgüngör
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Ir Spectrum ◽  
Polymeric Chain ◽  
X Ray Diffraction ◽  
Bimetallic Complex ◽  
One Dimensional ◽  
X Ray

AbstractThe cyano-bridged heteronuclear coordination polymer of zinc(II)/nickel(II) has been prepared by N-(2-hydroxyethyl)-ethylendiamine (hydet-en), alternatively named 2-(2-aminoethylamino)-ethanol and characterised by IR and thermal analysis. In the bimetallic complex, the decomposition of hydet-en ligands is seen to be endothermic whereas that of the cyano ligands is found to be exothermic. The crystal structure of the complex has been determined by single-crystal X-ray diffraction. The crystal structure of the zinc(II)-nickel(II) complex consists of a one-dimensional polymeric chain –Zn(hydet-en)

Lewis-Base Adducts of Group 1B Metal(I) Compounds. XXI The Crystal and Molecular Structures of the Unsolvated Forms of Dibromotris(triphenylphosphine)dicopper(I) and 'step' Tetrabromotetrakis(triphenyl-phosphine)tetracopper(I)

1985 ◽  
Vol 38 (8) ◽  
pp. 1243 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
C Pakawatchai ◽  
PC Healy ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Molecular Structures ◽  
Lewis Base ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triphenyl Phosphine ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal structures of the title compounds have been determined by single-crystal X-ray diffraction methods at 295 K. Crystal data for (PPh3)2CuBr2Cu(PPh3) (1) show that the crystals are iso-morphous with the previously studied chloro analogue, being monoclinic, P21/c, a 19.390(8), b 9.912(5), c 26.979(9) Ǻ, β 112,33(3)°; R 0.043 for No 3444. Cu( trigonal )- P;Br respectively are 2.191(3); 2.409(2), 2.364(2) Ǻ. Cu(tetrahedral)- P;Br respectively are 2.241(3), 2.249(3); 2.550(2), 2.571(2) Ǻ. Crystals of 'step' [PPh3CuBr]4 (2) are isomorphous with the solvated bromo and unsolvated iodo analogues, being monoclinic, C2/c, a 25.687(10), b 16.084(7), c 17.815(9) Ǻ, β 110.92(3)°; R 0.072 for No 3055. Cu( trigonal )- P;Br respectively are 2.206(5); 2.371(3), 2.427(2) Ǻ. Cu(tetrahedral)- P;Br are 2.207(4); 2.446(2), 2.676(3), 2.515(3) Ǻ.

scholarly journals A new Rubidium - Bismuth polyphosphate RbBi(PO3)4: Growth, X-ray single crystal and vibrational study

2014 ◽  
Vol 10 (7) ◽  
pp. 2881-2893
Author(s):  
Khaled JAOUADI ◽  
Tahar MHIRI ◽  
Nabil ZOUARI
Keyword(s):  
Single Crystal ◽  
Structural Type ◽  
Inorganic Materials ◽  
X Ray ◽  
Weighted Residuals ◽  
Type Iv ◽  
Anisotropic Temperature ◽  
Solution Studies ◽  
Bridge Oxygen ◽  
Temperature Factors

Solid-solution studies in the ternary Rb2O – Bi2O3 – P2O5 system, carried out in a search for inorganic materials have a considerable interest mainly for their optical properties, specifically in laser technology, yielded the new compound RbBi(PO3)4. Single-crystal X-ray measurement revealed that RbBi(PO3)4 crystallizes in space group P21/c with a structural type IV and has lattice parameters a = 10.430, b = 8.984, c = 12.967 Å,  = 126.1°, Z = 4 and V = 981.6 Å3. The all eighteen atoms were located in the asymmetric unit. Refinement using anisotropic temperature factors for all atoms yielded weighted residuals based on F and F2 values, respectively, of R1 = 0.0131 and WR2 = 0.0252 for all observed reflections. The atomic arrangement can be described as a long chain polyphosphate organization, helical ribbons (PO3)n. Two types of infinite chains, with a period of eight PO4 tetrahedra run along the longest unit-cell directions. Infrared and Raman spectra at room temperature, were investigated, show clearly some characteristics bands of infinite chains structure of PO4 tetrahedra linked by a bridge oxygen.

scholarly journals The Synthesis and Characterization of a Novel One-Dimensional Bismuth (III) Coordination Polymer as a Precursor for the Production of Bismuth (III) Oxide Nanorods

Crystals ◽  
2022 ◽  
Vol 12 (1) ◽  
pp. 113
Author(s):  
Younes Hanifehpour ◽  
Babak Mirtamizdoust ◽  
Jaber Dadashi ◽  
Ruiyao Wang ◽  
Mahboube Rezaei ◽  
...  
Keyword(s):  
Single Crystal ◽  
Coordination Compound ◽  
Organic Ligand ◽  
One Dimensional ◽  
X Ray ◽  
X Ray Crystallography ◽  
Oxide Nanorods ◽  
Pure Phase ◽  
3D Framework

A novel Bi (III) coordination compound, [Bi(HQ)(Cl)4]n ((Q = pyridine-4-carbaldehyde thiosemicarbazone), was prepared in this research using a sonochemical technique. SEM, infrared spectroscopy (IR), XRD, and single-crystal X-ray analysis were utilized to analyze the Bi(III) coordination compound. The structure determined using single-crystal X-ray crystallography indicates that the coordination compound is a 1D polymer in solid state and that the coordination number of bismuth (III) ions is six, (BiSCl5), with one S donor from the organic ligand and five Cl donors from anions. It is equipped with a hemidirectional coordination sphere. It is interesting that the ligand has been protonated in the course of the reaction with a Cl- ion balancing the charge. This compound’s supramolecular properties are directed and regulated by weak directional intermolecular interactions. Through π–π stacking interactions, the chains interact with one another, forming a 3D framework. Thermolysis of the compound at 170 °C with oleic acid resulted in the formation of pure phase nanosized Bi (III) oxide. SEM technique was used to examine the morphology and size of the bismuth (III) oxide product produced.

Structural Systematics of 2/4-Nitrophenoxide Complexes of Closed-Shell Metal Ions. V 2-Nitrophenoxides of Group 2

1998 ◽  
Vol 51 (8) ◽  
pp. 761 ◽  
Author(s):  
Jack M. Harrowfield ◽  
Raj Pal Sharma ◽  
Brian W. Skelton ◽  
Allan H. White
Keyword(s):  
Water Molecule ◽  
Metal Ions ◽  
Single Crystal ◽  
Room Temperature ◽  
Closed Shell ◽  
Magnesium Salt ◽  
Water Molecules ◽  
One Dimensional ◽  
X Ray ◽  
Group 2

Room-temperature single-crystal X-ray studies are recorded for 2-nitrophenoxide salts of Group 2 metals, variously hydrated M(2-np)2.xH2O, M = Mg, Ca, Sr; the structure of the barium analogue has been previously recorded. Mg(2-np)2.2H2O is monoclinic, P21/a, a 7·377(1), b 7·518(1), c 12·877(3) Å, β 106·58(2)°, Z = 2; conventional R on |F| 0·13 for No 508 independent ‘observed’ (I > 3σ(I)) reflections. Ca(2-np)2.H2O is monoclinic, C2, a 25·92(1), b 7·176(3), c 3·660(4) Å, β 93·66(5)°, Z = 2, R 0·061 for No 541. M(2-np)2.4H2O, M = Ca, Sr, are isomorphous, monoclinic, C2/c, a ≈ 31·3, b ≈ 8·1, c ≈ 12·8 Å, β 103°, Z = 8; R was 0·056, 0·055 forNo 1988, 1744 respectively. The magnesium salt is a discrete molecular array disposed about a crystallographic inversion centre with chelating phenoxide ligands: trans-[Mg(2-np)2(OH2)2]. The calcium monohydrate salt is a novel one-dimensional polymer with a ... Ca(µ-O)2Ca(µ-O)2Ca ... spine, the ligand pairs chelating the calcium with phenoxide-O additionally bridging. The seven-coordinate calcium atoms lie on the crystallographic 2 axis with the water molecule, also on that axis, making up a seven-coordinate environment. The tetrahydrate is also a one-dimensional polymer with a similar spine, the bridging oxygen atoms derivative of water molecules. A chelating ligand and two further water molecules make up an eight-coordinate metal environment, with the free anions interleaving stacks of coordinated anions up c.

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